CN107201513A - A kind of pretreatment of metal surface liquid and its application based on tannic acid for the Phosphateless environmentally friendly of main film forming substance - Google Patents
A kind of pretreatment of metal surface liquid and its application based on tannic acid for the Phosphateless environmentally friendly of main film forming substance Download PDFInfo
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- CN107201513A CN107201513A CN201710406660.3A CN201710406660A CN107201513A CN 107201513 A CN107201513 A CN 107201513A CN 201710406660 A CN201710406660 A CN 201710406660A CN 107201513 A CN107201513 A CN 107201513A
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- metal surface
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- tannic acid
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/50—Treatment of iron or alloys based thereon
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Abstract
The present invention relates to a kind of pretreatment of metal surface liquid based on tannic acid for the Phosphateless environmentally friendly of main film forming substance and its application, it is as follows that the pretreatment fluid includes material quality percentage：Tannic acid 0.1~0.3%, inhibitor component 0.2~0.5%, zinc nitrate 0.3~0.5%, sodium gluconate 0.1~0.5%, sodium tartrate 0.01~0.04%, surplus is water.Pretreatment of metal surface formula of liquid contained substance species of the present invention is less, prepares simple, uses material not contain the harmful substances such as phosphorus, chromium, be a kind of prescription for the treatment of liquid of environmental protection and economy.Film surface pattern relative coarseness after pretreatment of metal surface liquid of the present invention processing, and containing substantial amounts of oh group, greatly enhance the adhesion with paint film.
Description
Technical field
The present invention relates to a kind of pretreatment of metal surface liquid using tannic acid as the Phosphateless environmentally friendly of main film forming substance and its
Using belonging to metal conditioner technical field.
Background technology
At present, most widely used metal surface treatment technology is phosphorization treatment technology in industrial production：By metallic substrates
In containing manganese, iron zinc, the phosphate solution of calcium, it is chemically treated, one layer of its Surface Creation is insoluble in the porous of water
The binding ability of phosphate coating, enhancing metallic substrates and paint film.But the waste liquid sediment produced in parkerizing process can be brought
Serious problem of environmental pollution.To adapt to the requirement of environmental protection, a kind of without phosphorus environment-friendly Treatment of Metal Surface is developed
Liquid replaces the traditional phosphating solution used at present to be significant.
Tannic acid belongs to hydrolysable tannins, is the natural products with important value of exploiting and utilizing.It has multiple ortho position phenol
Hydroxyl structure, can occur complex reaction as a kind of multidentate ligand and metal ion, form the complex with network structure
Film layer, in water treatment field, the hardness of water, and passive metal substrate is reduced available for scale remover, strengthens corrosion stability.In addition,
Tannic acid does not contain P elements, it is to avoid a series of problem brought in phosphatization production process, such as waste liquid sediment, water body richness battalion
Fosterization etc..This characteristic based on tannic acid, is developed at the environmentally friendly metal surface by main film forming substance of tannic acid
Reason liquid is significant and good application prospect.
Chinese patent document CN105779986A (application numbers：201610277768.2) disclose a kind of naked steel surface of coating
Acid rain resistant corrosive agent and preparation method thereof, the raw materials by weight meter of the acid rain resistant corrosive agent includes 1~3%
NaHSO3, 0.5~2% copper sulphate, 1~3% sodium tripolyphosphate, 1~3% sodium molybdate, 0.1~0.5% phytic acid and
0.1~0.5% tannic acid；Its surplus is water.By NaHSO3, copper sulphate, sodium tripolyphosphate, sodium molybdate, phytic acid, tannic acid and water
It is well mixed, that is, prepare acid rain resistant corrosive agent.But sodium tripolyphosphate is with the addition of in this acid rain resistant corrosive agent, due to inorganic
The presence of P elements, the discharge of waste liquid can cause the eutrophication of water body.In addition its dominant mechanism is to form one in metal surface
The protective rust of individual stability, the adhesion with external coating (as painted) is weaker, is unfavorable for after-treatment application, limits it
Using.
The content of the invention
In view of the shortcomings of the prior art, especially present in prior art phosphorus pollution and poor film adhesion not
Foot, the present invention provides a kind of environment-friendly metal surface treating liquid based on tannic acid with preferable etch resistant properties, at this
The main chemical composition coating for building densification in metal surface by main film forming substance of tannic acid of liquid is managed, it is anti-with preferable corrosion
Performance, and its coarse surface structure are protected, with substantial amounts of oh group, film adhesion is significantly enhanced, is a kind of ring
Protect economic chemical composition coating.
Technical scheme is as follows：
A kind of pretreatment of metal surface liquid based on the Phosphateless environmentally friendly that tannic acid is main film forming substance, including material quality
Percentage is as follows：
Tannic acid 0.1~0.3%, inhibitor component 0.2~0.5%, zinc nitrate 0.3~0.5%, sodium gluconate 0.1
~0.5%, sodium tartrate 0.01~0.04%, surplus is water.
It is described pre- for the metal surface of the Phosphateless environmentally friendly of main film forming substance based on tannic acid according to currently preferred
Treatment fluid, including material quality percentage are as follows：
Tannic acid 0.15~0.2%, inhibitor component 0.3~0.4%, zinc nitrate 0.35~0.4%, sodium gluconate
0.1~0.2%, sodium tartrate 0.01~0.02%, surplus is water.
It is described pre- for the metal surface of the Phosphateless environmentally friendly of main film forming substance based on tannic acid according to currently preferred
Treatment fluid, including material quality percentage are as follows：
Tannic acid 0.15%, inhibitor component 0.3%, zinc nitrate 0.4%, sodium gluconate 0.1%, sodium tartrate
0.01%, surplus is water.
It is described pre- for the metal surface of the Phosphateless environmentally friendly of main film forming substance based on tannic acid according to currently preferred
Treatment fluid, including material quality percentage are as follows：
Tannic acid 0.18%, inhibitor component 0.3%, zinc nitrate 0.35%, sodium gluconate 0.15%, sodium tartrate
0.01%, surplus is water.
It is described pre- for the metal surface of the Phosphateless environmentally friendly of main film forming substance based on tannic acid according to currently preferred
Treatment fluid, including material quality percentage are as follows：
Tannic acid 0.20%, inhibitor component 0.35%, zinc nitrate 0.35%, sodium gluconate 0.2%, sodium tartrate
0.02%, surplus is water.
It is described pre- for the metal surface of the Phosphateless environmentally friendly of main film forming substance based on tannic acid according to currently preferred
PH=4.0~5.0 for the treatment of fluid, further preferred pH=4.0~4.5.
The pretreatment of metal surface liquid of the present invention is slightly yellow transparency liquid, and pH is between 4.0~5.0.Metallic article is such as
Cold-reduced sheet is after degreasing degreasing is handled, and advanced water-filling is washed, and is then surface-treated, and the time is 3~6 minutes, can be in metal
Surface obtains uniform blue film layer.
According to the present invention, the above-mentioned pretreatment of metal surface liquid based on tannic acid for the Phosphateless environmentally friendly of main film forming substance exists
Application in pretreatment of metal surface, including step are as follows：
Pending metal surface is first subjected to ungrease treatment, washed again after metal surface greasy dirt is eliminated, then
Metal is placed in the pretreatment of metal surface liquid of pH=4~5.0 and handled 3~6 minutes, then taken out and dried in the air in natural environment
Dry or drying, that is, complete Treatment of Metal Surface.
Application according to the present invention, it is preferred that processing time is 4 minutes.
PH should be maintained between 4.0~5.0 the pretreatment of metal surface liquid of the present invention in use, the place newly prepared
Liquid pH value is managed 4.2 or so, as processing workpiece increases, pH can gradually increase, and after pH value is more than 5.0, film forming is uneven.
Processing time should be maintained at 3-6min, when treated between be less than 3min when, Film color is shallower and uneven.Between when treated
During higher than 6min or when the time is longer, iron plate can produce the corrosion of small degree, and optimal film formation time is 4min.
The principle of the present invention is as follows：
Tannic acid has multiple ortho position phenolic hydroxyl structures, can occur complexing as a kind of multidentate ligand and metal ion anti-
Should.In the present invention, tannic acid, can be with Zn as a kind of film forming matter2+Generation complexation reaction forms nano particle, is dispersed in place
Manage in liquid.When iron-based bottom is immersed in treatment fluid, because sour environment iron-based basal surface can produce one layer of Fe2+, substrate table
Complex reaction occurs for the phenolic hydroxyl group that the iron ion in face can contain with the tannic acid in treatment fluid, and tannic acid molecule is assembled into metal
Surface.Then, the nano particle in solution can be deposited on metal surface, and using zinc ion as a bridging material, make film
Layer continued growth on three-dimensional, obtains the chemical composition coating based on tannic acid Yu metal ion macromolecular complex thing.It has
There are two aspect advantages, on the one hand it can strengthen the corrosion stability of metallic substrates, on the other hand substantial amounts of hydroxyl base is contained on its surface
Group, can strengthen the binding ability with external coating.
Inhibitor component is a kind of polymer molecule of synthesis, and it can form stable chemical combination with metal ion, calcium, magnesium etc.
Thing, available for antisludging agent, while it is also a kind of dispersant.Iron-based basal surface can be adsorbed onto in metal treatment fluid, also may be used
It is crosslinked with tannin acid molecule by zinc ion.
Zinc nitrate can connect different tannin acid molecules in two dimension and three dimensions, formed as a bridging agent
Multilayer film self assembly.
Sodium gluconate is a kind of corrosion inhibiter, can for strengthen metallic substrates corrosion resistance.
On the one hand tartaric acid make film forming more uniform as a kind of complexing agent, on the other hand can prevent metallic substrates table
The problems such as face is because there is dust causes film adhesion to be deteriorated.
Compared with prior art, the present invention has advantages below：
1st, pretreatment of metal surface formula of liquid contained substance species of the present invention is less, prepares simple, uses material not
It is a kind of prescription for the treatment of liquid of environmental protection and economy containing harmful substances such as phosphorus, chromium.
2nd, pretreatment of metal surface liquid of the present invention application process operation it is fairly simple, and can with passivation substrate and formed compared with
Good corrosion stability film layer.
3rd, the film surface pattern relative coarseness after pretreatment of metal surface liquid of the present invention processing, and containing substantial amounts of
Hydroxyl
Group, greatly enhances the adhesion with paint film.By after pretreatment of metal surface liquid of the present invention processing
Cold-reduced sheet enters
The lattice of row hundred are tested, and its adhesive force grade can reach zero level.Cold-reduced sheet 80N/cm2Power carry out impulsive force examination
After testing,
Front, the back side are "dead", and crackle occurs.
Brief description of the drawings
Fig. 1 is the cold-reduced sheet outside drawing after pretreatment of metal surface liquid processing in the embodiment of the present invention 1.
Fig. 2 is (former for the AFM of cold-reduced sheet surface microscopic topographic after pretreatment of metal surface liquid processing in the embodiment of the present invention 1
Sub- force microscope) picture.
Fig. 3 is cold rolling plate surface EDS (energy disperse spectroscopy) elemental map after pretreatment of metal surface liquid processing in the embodiment of the present invention 1
Piece.
Embodiment
Below by specific embodiment, the present invention will be further described, but not limited to this.
Raw material described in embodiment is convenient source, commercial products.
Embodiment 1
A kind of pretreatment of metal surface liquid based on the Phosphateless environmentally friendly that tannic acid is main film forming substance, material quality percentage
Than as follows：
Tannic acid 0.15%, inhibitor component 0.3%, zinc nitrate 0.4%, sodium gluconate 0.1%, sodium tartrate
0.01%, surplus is water.
The treatment fluid of the present embodiment is prepared cold rolling plate surface handled after (pH=4.4), step is as follows：
(1) degreasing degreasing, washing are carried out to cold rolling plate surface；
(2) cold-reduced sheet after step (1) processing is placed in immersion treatment 4 minutes in treatment fluid under normal temperature；
(3) it will be dried after the cold-reduced sheet washing after step (2) processing, that is, complete surface treatment.
Cold-reduced sheet outside drawing in the present embodiment after the processing of pretreatment of metal surface liquid, as shown in figure 1, as shown in Figure 1, warp
The metal surface crossed after processing obtains uniform blue film layer.
The AFM (AFM) of cold-reduced sheet surface microscopic topographic after pretreatment of metal surface liquid is handled in the present embodiment
Picture, as shown in Figure 2.As shown in Figure 2, metal surface after treatment is mainly an aggregation of nanometer spherical particle,
It is uneven, with larger surface roughness, it can greatly strengthen the binding ability with external coating.
Cold rolling plate surface EDS (energy disperse spectroscopy) element picture after the processing of pretreatment of metal surface liquid in the present embodiment, such as Fig. 3 institutes
Show, each element ratio is as shown in table 1.From Fig. 3 and table 1, the iron-based basal surface after processing mainly contains C, O, Zn, Fe member
Element, Zn-ef ficiency take part in the formation of iron-based basal surface film as a bridging agent molecule.
Table 1
Embodiment 2
A kind of pretreatment of metal surface liquid based on the Phosphateless environmentally friendly that tannic acid is main film forming substance, material quality percentage
Than as follows：
Tannic acid 0.18%, inhibitor component 0.3%, zinc nitrate 0.35%, sodium gluconate 0.15%, sodium tartrate
0.01%, surplus is water.
The treatment fluid of the present embodiment is prepared cold rolling plate surface handled after (pH=4.2), step is as follows：
(1) degreasing degreasing, washing are carried out to cold rolling plate surface；
(2) cold-reduced sheet after step (1) processing is placed in immersion treatment 4 minutes in treatment fluid under normal temperature；
(3) it will be dried after the cold-reduced sheet washing after step (2) processing, that is, complete surface treatment.
Embodiment 3
A kind of pretreatment of metal surface liquid based on the Phosphateless environmentally friendly that tannic acid is main film forming substance, material quality percentage
Than as follows：
Tannic acid 0.20%, inhibitor component 0.35%, zinc nitrate 0.35%, sodium gluconate 0.2%, sodium tartrate
0.02%, surplus is water.
The treatment fluid of the present embodiment is prepared cold rolling plate surface handled after (pH=4.5), step is as follows：
(1) degreasing degreasing, washing are carried out to cold rolling plate surface；
(2) cold-reduced sheet after step (1) processing is placed in immersion treatment 4 minutes in treatment fluid under normal temperature；
(3) it will be dried after the cold-reduced sheet washing after step (2) processing, that is, complete surface treatment.
Comparative example 1, tannic acid consumption are excessive
A kind of pretreatment of metal surface liquid based on the Phosphateless environmentally friendly that tannic acid is main film forming substance, material quality percentage
Than as follows：
Tannic acid 1%, inhibitor component 0.3%, zinc nitrate 0.4%, sodium gluconate 0.1%, sodium tartrate 0.01%,
Surplus is water.
Process step be the same as Example 1 is carried out to cold rolling plate surface.
Comparative example 2, tannic acid consumption are too low
A kind of pretreatment of metal surface liquid based on the Phosphateless environmentally friendly that tannic acid is main film forming substance, material quality percentage
Than as follows：
Tannic acid 0.05%, inhibitor component 0.3%, zinc nitrate 0.4%, sodium gluconate 0.1%, sodium tartrate
0.01%, surplus is water.
Process step be the same as Example 1 is carried out to cold rolling plate surface.
Comparative example 3, without tannic acid
A kind of pretreatment of metal surface liquid based on the Phosphateless environmentally friendly that tannic acid is main film forming substance, material quality percentage
Than as follows：
Inhibitor component 0.3%, zinc nitrate 0.4%, sodium gluconate 0.1%, sodium tartrate 0.01%, surplus is water.
Process step be the same as Example 1 is carried out to cold rolling plate surface.
Test example
Performance detection, test event and knot are carried out to the cold-reduced sheet after the surface treatment in embodiment 1-3 and comparative example 1-3
Fruit is as follows：
(a) the cold-reduced sheet outward appearance after liquid processing processed by the invention is observed：
Embodiment 1-3：Cold-reduced sheet is after processing, and surface generates one layer of uniform light blue chemical composition coating.
Comparative example 1-3：Comparative example 1 is one layer of blue yellow chemical composition coating of generation, has slight corrosion, comparative example 2-3 makes a living
Into one layer of light blue chemical composition coating, film forming color is especially shallow.
(b) copper sulphate drop is tested：Copper-bath is prepared according to national standard：
CuSO4·5H2O：41g/L；
NaCl：35g/L；
0.1mol/L HCl：13mL/L.
The copper sulphate titration time of cold-reduced sheet after liquid processing processed by the invention：
Embodiment 1：60 seconds, embodiment 2：65 seconds, embodiment 3：55 seconds.
Comparative example 1：35 seconds, comparative example 2：45 seconds, comparative example 3：38 seconds.
(c) 3.5wt% brine soaking experiments：
Brine soaking experiment of the cold-reduced sheet through the processing of present treatment liquid in 3.5wt%：
Embodiment 1：Do not occur a large amount of rust spots in 50 minutes
Embodiment 2：Do not occur a large amount of rust spots in 55 minutes
Embodiment 3：Do not occur a large amount of rust spots in 45 minutes
Comparative example 1：Do not occur a large amount of rust spots in 25 minutes
Comparative example 2：Do not occur a large amount of rust spots in 35 minutes
Comparative example 3：Do not occur a large amount of rust spots in 30 minutes
The embodiment 1-3 saline sook times are all up to state standards, and the comparative example 1-3 saline sook times substantially shorten.
(d) paint film adhesion is tested：The cold-reduced sheet handled in embodiment 1-3 and comparative example 1-3 is carried out at electrostatic dusting
After reason, the test of paint film adhesion is carried out.
Draw lattice experiment：The cold-reduced sheet after embodiment 1-3 processing is subjected to hundred lattice experiments, its adhesive force grade using hundred lattice devices
Zero level can be reached.
The cold-reduced sheet after comparative example 1-3 processing is subjected to hundred lattice experiments using hundred lattice devices, its adhesive force grade can be reached
Three-level.
Anti-impact force is tested：Cold-reduced sheet after embodiment 1-3 processing carries out impulsive force experiment with 80N/cm2 power
Afterwards, the "dead" crackle in front, the back side occurs.
The cold-reduced sheet after example 1-3 processing is carried out after impulsive force experiment with 80N/cm2 power by contrast, and front, the back side are equal
There is radioactivity crackle.
Claims (8)
1. it is a kind of based on pretreatment of metal surface liquid of the tannic acid for the Phosphateless environmentally friendly of main film forming substance, it is characterised in that should
It is as follows that pretreatment fluid includes material quality percentage：
Tannic acid 0.1~0.3%, inhibitor component 0.2~0.5%, zinc nitrate 0.3~0.5%, sodium gluconate 0.1~
0.5%, sodium tartrate 0.01~0.04%, surplus is water.
2. it is according to claim 1 based on pretreatment of metal surface of the tannic acid for the Phosphateless environmentally friendly of main film forming substance
Liquid, it is characterised in that it is as follows that the pretreatment fluid includes material quality percentage：
Tannic acid 0.15~0.2%, inhibitor component 0.3~0.4%, zinc nitrate 0.35~0.4%, sodium gluconate 0.1~
0.2%, sodium tartrate 0.01~0.02%, surplus is water.
3. it is according to claim 1 based on pretreatment of metal surface of the tannic acid for the Phosphateless environmentally friendly of main film forming substance
Liquid, it is characterised in that it is as follows that the pretreatment fluid includes material quality percentage：
Tannic acid 0.15%, inhibitor component 0.3%, zinc nitrate 0.4%, sodium gluconate 0.1%, sodium tartrate 0.01%,
Surplus is water.
4. it is according to claim 1 based on pretreatment of metal surface of the tannic acid for the Phosphateless environmentally friendly of main film forming substance
Liquid, it is characterised in that it is as follows that the pretreatment fluid includes material quality percentage：
Tannic acid 0.18%, inhibitor component 0.3%, zinc nitrate 0.35%, sodium gluconate 0.15%, sodium tartrate
0.01%, surplus is water.
5. it is according to claim 1 based on pretreatment of metal surface of the tannic acid for the Phosphateless environmentally friendly of main film forming substance
Liquid, it is characterised in that it is as follows that the pretreatment fluid includes material quality percentage：
Tannic acid 0.20%, inhibitor component 0.35%, zinc nitrate 0.35%, sodium gluconate 0.2%, sodium tartrate
0.02%, surplus is water.
6. it is according to claim 1 based on pretreatment of metal surface of the tannic acid for the Phosphateless environmentally friendly of main film forming substance
Liquid, it is characterised in that pH=4.0~5.0 of the pretreatment fluid.
7. the pretreatment of metal surface liquid based on the Phosphateless environmentally friendly that tannic acid is main film forming substance described in claim 1 is in gold
Application in metal surface pretreatment, including step are as follows：
Pending metal surface is first subjected to ungrease treatment, washed again after metal surface greasy dirt is eliminated, then by gold
Category be placed in the pretreatment of metal surface liquid of pH=4~5.0 handle 3~6 minutes, then take out and dried in natural environment or
Drying, that is, complete Treatment of Metal Surface.
8. application according to claim 7, it is characterised in that locate in advance the metal surface that metal is placed on pH=4~5.0
It is 4 minutes to manage processing time in liquid.
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| CN111235576A (en) * | 2020-01-15 | 2020-06-05 | 浙江大学 | Method for constructing micro-nano porous organic acid pretreatment layer on metal surface and application |
| CN114717543A (en) * | 2022-03-12 | 2022-07-08 | 浙江五源科技股份有限公司 | Preparation method of composition for improving salt spray resistance of coating after iron and steel non-phosphorus conversion treatment |
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| CN111235576A (en) * | 2020-01-15 | 2020-06-05 | 浙江大学 | Method for constructing micro-nano porous organic acid pretreatment layer on metal surface and application |
| WO2021143551A1 (en) * | 2020-01-15 | 2021-07-22 | 浙江大学 | Method of forming micro/nanoporous organic acid pre-treatment layer on metal surface, and application |
| CN114717543A (en) * | 2022-03-12 | 2022-07-08 | 浙江五源科技股份有限公司 | Preparation method of composition for improving salt spray resistance of coating after iron and steel non-phosphorus conversion treatment |
| CN114717543B (en) * | 2022-03-12 | 2023-06-09 | 浙江五源科技股份有限公司 | Preparation method of composition for improving salt spray resistance of coating after non-phosphorus conversion treatment of steel |
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| CN107201513B (en) | 2019-03-19 |
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